CN106315629A - Technology for preparing high-purity lithium carbonate through recovering of battery-grade lithium carbonate lithium precipitation mother liquor - Google Patents
Technology for preparing high-purity lithium carbonate through recovering of battery-grade lithium carbonate lithium precipitation mother liquor Download PDFInfo
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- CN106315629A CN106315629A CN201610759250.2A CN201610759250A CN106315629A CN 106315629 A CN106315629 A CN 106315629A CN 201610759250 A CN201610759250 A CN 201610759250A CN 106315629 A CN106315629 A CN 106315629A
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- lithium
- lithium carbonate
- sinker
- mother liquor
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/08—Carbonates; Bicarbonates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The invention provides a technology for preparing high-purity lithium carbonate through recovering of battery-grade lithium carbonate lithium precipitation mother liquor. The technology comprises acidification, fluorination lithium precipitation, slurry blending and caustification, a hydrogenation reaction, lithium precipitation through pyrolysis and other technological steps, wherein in the fluorination lithium precipitation step, sodium fluoride is added to acidified lithium precipitation mother liquor for a lithium precipitation reaction, lithium fluoride residues are obtained, correspondingly, in the slurry blending and caustification step, water and calcium hydroxide are added to the lithium fluoride residues, a lithium hydroxide solution is obtained and subjected to a hydrogenation reaction and lithium precipitation through pyrolysis, and high-purity lithium carbonate is obtained. In the technology for preparing high-purity lithium carbonate through recovering of the battery-grade lithium carbonate lithium precipitation mother liquor, high-purity lithium carbonate is prepared directly from lithium hydroxide, the lithium precipitation mother liquor is not required to be returned to an original system, industrial-grade lithium carbonate is prepared firstly, then high-purity lithium carbonate is prepared after lithium hydroxide is obtained through caustification of industrial-grade lithium carbonate, and the technology is simple, low in cost, considerable in economic benefit and suitable for industrial application.
Description
Technical field
The present invention relates to the recovery technology field of sinker mother solution, particularly relate to one and utilize battery-level lithium carbonate sinker mother solution
The technique reclaiming preparation pure Lithium Carbonate.
Background technology
Lithium carbonate is the basic material of lithium salts industry, has multiple industrial use, is possible not only to directly use, it is also possible to as
Raw material prepares the high lithium salts of various added value and compound thereof, is widely used in battery industry, ceramics, glass industry, aluminum work
The fields such as industry, lubricant, cold-producing medium, nuclear industry and photovoltaic industry.Wherein, battery industry mainly uses battery-level lithium carbonate next life
Produce the positive electrode of the lithium ion batteries such as cobalt acid lithium, LiFePO4, lithium nickelate, LiMn2O4, ternary material, nickle cobalt lithium manganate.
The preparation of battery-level lithium carbonate is typically with Li2SO4For raw material, use soda sinker, after sinker, Li+With Li2CO3's
Mode precipitates, but still suffers from a small amount of Li in solution+, this solution is referred to as sinker mother solution.Li in sinker mother solution+Recycling
It it is one of the key issue of lithium carbonate preparation technology.At present, the recovery and treatment method of sinker mother solution is usually: in sinker mother solution
Being initially charged sulphuric acid to neutralize, re-evaporation concentrates, and isolates sodium sulfate, then mother solution returns sinker system；Sink owing to mother solution returns
Lithium system can cause the accumulation of impurity, therefore, the Li in sinker mother solution+Finally it is produced out with the form of technical grade lithium carbonate
Coming, pure Lithium Carbonate to be obtained needs to purify refined further for technical grade lithium carbonate, first prepares technical grade lithium carbonate, then from
The technological process that technical grade lithium carbonate prepares pure Lithium Carbonate is complicated, relatively costly.Along with aluminium lithium alloy, lithium battery, nuclear fusion
Deng high speed development and a series of policy about development new-energy automobile of country's appearance of high-technology field, prepare high-end carbon
Acid lithium meets the growing market demand and is particularly important, and utilizes battery-level lithium carbonate sinker disposing mother liquor as one
The technical meaning of preparation pure Lithium Carbonate is the most great.
Summary of the invention
It is an object of the invention to, overcome prior art to be worth not only with the sinker mother solution preparation of battery-level lithium carbonate
The technological deficiency of high technical grade lithium carbonate, it is provided that one utilizes battery-level lithium carbonate sinker disposing mother liquor to prepare pure Lithium Carbonate
Technique.
For solving above-mentioned technical problem, the technical scheme is that offer one utilizes battery-level lithium carbonate sinker female
Liquid reclaims the technique of preparation pure Lithium Carbonate, and described process program is carried out as follows:
S101: acidifying: add sulphuric acid in sinker mother solution, regulate PH=2-5, be subsequently adding liquid caustic soda or solid caustic soda, regulate PH=
7-8；
Adding sulphuric acid in sinker mother solution and drive away carbon dioxide, when adding sulphuric acid, control pH value is between 2-5, meeting when pH value is too low
Wasting more sulphuric acid and liquid caustic soda or Caustic soda, the too high meeting of pH value makes to react insufficient, causes lithium yield low.
S102: fluorination sinker: add sodium fluoride in the solution in described step S101 and carry out sinker reaction, the most liquid-solid
Separate, obtain lithium fluoride slag；
[w1] utilizes the strong oxidizing property of fluorine element and the strong reducing property of elemental lithium, generates lithium fluoride precipitation, and its reaction equation is:
F-+Li+=LiF
S103: causticization of sizing mixing: add pure water in described lithium fluoride slag and size mixing, add calcium hydroxide after sizing mixing and carry out causticization
Reaction, then filters, and obtains lithium hydroxide solution；
Preparation pure Lithium Carbonate first has to obtain Lithium hydrate or lithium bicarbonate, herein, lithium fluoride in water with calcium hydroxide
React, generate lithium hydroxide solution and calcium fluoride precipitate, lithium hydroxide solution after filtration, can be obtained.
S104: hydrogenation: be passed through carbon dioxide in described lithium hydroxide solution and carry out hydrogenation, obtain bicarbonate
Lithium solution；
The dissolubility of lithium bicarbonate is relatively big, and the impurity in Lithium hydrate is (such as Ca2+、Mg2+Deng) be not hydrogenated, with insoluble carbonic acid
Presented in salt, can be filtered to remove, improve the purity of lithium carbonate.
S105: Thermal desorption lithium: by described lithia water heat resolve, separates out pure Lithium Carbonate.
Lithium bicarbonate heat resolve, its decomposition reaction formula is as follows:
2LiHCO3→Li2CO3+H2O+CO2
Preferably, described step S102 adds the amount of sodium fluoride than Li in the solution of described step S101+Content excess 5%-
8%。
Add the sodium fluoride of excess, to ensure that lithium ion, all presented in lithium fluoride precipitates, improves the response rate of lithium,
But excess can cause the wasting of resources too much, it is advisable with excess 5%-8%.
Preferably, the pure water added in described step S103 is 20-30:1 with the liquid-solid ratio of lithium fluoride slag.
In lithium fluoride slag, add the water of excess, to ensure that lithium fluoride slag and calcium salt can fully react, make lithium fluoride slag
In lithium ion fully dissolve, improve lithium the response rate.The water added the most then affects the response rate of lithium, the most then money of wasting water
Source, is advisable with liquid-solid ratio for 20-30:1.
Preferably, in described step S105, heating-up temperature is more than 90 DEG C.
Decompose after lithia water heating, when heating-up temperature is more than 90 DEG C, LiHCO3Decomposition rate sharply increases,
Therefore, general pyrolysis temperature controls more than 90 DEG C, with the time of saving.
The technical scheme that embodiments of the invention provide can include following beneficial effect:
The present invention provides a kind of technique utilizing battery-level lithium carbonate sinker disposing mother liquor to prepare pure Lithium Carbonate, including acidifying,
The processing steps such as fluorination sinker, causticization of sizing mixing, hydrogenation, Thermal desorption lithium, wherein, in described fluorination sinker step after acidifying
Sinker mother solution in add sodium fluoride and carry out sinker reaction, it is thus achieved that lithium fluoride slag, accordingly, described in size mixing in causticization step to institute
State and lithium fluoride slag adds water and calcium hydroxide, it is thus achieved that lithium hydroxide solution, be then passed through hydrogenation and Thermal desorption lithium obtains
Pure Lithium Carbonate.In the technique preparing pure Lithium Carbonate with battery-level lithium carbonate sinker disposing mother liquor that the present invention provides, directly
Sinker mother solution after acidifying adds sodium fluoride, utilizes the strong oxidizing property of fluorine element and the strong reducing property of elemental lithium, generate fluorine
Change lithium precipitation, then obtain Lithium hydrate through reactions such as causticizations, by Lithium hydrate direct preparation of high-purity lithium carbonate, it is not necessary to will be heavy
Lithium mother solution returns original system and first prepares technical grade lithium carbonate, then by technical grade lithium carbonate preparation height after causticization obtains Lithium hydrate
Pure lithium carbonate, technique is simple, and low cost has been broken and prepared the other lithium carbonate of lower level only with LITHIUM BATTERY sinker mother solution at present
Commercial routes, and prepare the pure Lithium Carbonate of wellr sold and in short supply higher value, economic benefits, be suitable for industrial applications.
Accompanying drawing explanation
In order to be illustrated more clearly that disclosure embodiment or technical scheme of the prior art, below will be to embodiment or existing
In having technology to describe, the required accompanying drawing used is briefly described, it should be apparent that, for those of ordinary skill in the art
Speech, on the premise of not paying creative work, it is also possible to obtain other accompanying drawing according to these accompanying drawings.
Fig. 1 is that the one that the embodiment of the present invention provides utilizes battery-level lithium carbonate sinker disposing mother liquor to prepare pure Lithium Carbonate
Process method flow chart.
Detailed description of the invention
For the technical scheme making those skilled in the art be more fully understood that in the present invention, real below in conjunction with the present invention
Execute the accompanying drawing in example, the technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that described enforcement
Example is only a part of embodiment of the present invention rather than whole embodiments.Based on the embodiment in the present invention, this area is common
The every other embodiment that technical staff is obtained under not making creative work premise, all should belong to present invention protection
Scope.
Seeing Fig. 1, the one provided for the embodiment of the present invention utilizes battery-level lithium carbonate sinker disposing mother liquor to prepare high-purity
The process schematic flow sheet of lithium carbonate, utilizes battery-level lithium carbonate sinker disposing mother liquor to prepare high-purity carbon in following example
The technique of acid lithium is all based on the method flow shown in Fig. 1.
Embodiment 1
The present embodiment provides a kind of technique utilizing battery-level lithium carbonate sinker disposing mother liquor to prepare pure Lithium Carbonate, described technique
Method flow is as it is shown in figure 1, carry out in accordance with the following steps:
S101: acidifying: add sulphuric acid in sinker mother solution, regulation, to PH=2, is subsequently adding liquid caustic soda, regulates to PH=7；
S102: fluorination sinker: the sodium fluoride adding excess 5% in the solution in described step S101 carries out sinker reaction, then
Solid-liquor separation, obtains lithium fluoride slag；
S103: causticization of sizing mixing: adding pure water in described lithium fluoride slag and size mixing, the pure water of addition is liquid-solid with lithium fluoride slag
Ratio is 20:1, adds calcium hydroxide and carries out causticizing reaction, then filter, obtain lithium hydroxide solution after sizing mixing；
S104: hydrogenation: be passed through carbon dioxide in described lithium hydroxide solution and carry out hydrogenation, obtain lithium bicarbonate molten
Liquid；
S105: Thermal desorption lithium: described lithia water heating 95 DEG C is decomposed, separates out pure Lithium Carbonate.
Embodiment 2
The present embodiment provides a kind of technique utilizing battery-level lithium carbonate sinker disposing mother liquor to prepare pure Lithium Carbonate, described technique
Method flow is as it is shown in figure 1, carry out in accordance with the following steps:
S101: acidifying: add sulphuric acid in sinker mother solution, regulation, to PH=5, is subsequently adding liquid caustic soda, regulates to PH=8；
S102: fluorination sinker: the sodium fluoride adding excess 8% in the solution in described step S101 carries out sinker reaction, then
Solid-liquor separation, obtains lithium fluoride slag；
S103: causticization of sizing mixing: adding pure water in described lithium fluoride slag and size mixing, the pure water of addition is liquid-solid with lithium fluoride slag
Ratio is 25:1, adds calcium hydroxide and carries out causticizing reaction, then filter, obtain lithium hydroxide solution after sizing mixing；
S104: hydrogenation: be passed through carbon dioxide in described lithium hydroxide solution and carry out hydrogenation, obtain lithium bicarbonate molten
Liquid；
S105: Thermal desorption lithium: described lithia water heating 98 DEG C is decomposed, separates out pure Lithium Carbonate.
Embodiment 3
The present embodiment provides a kind of technique utilizing battery-level lithium carbonate sinker disposing mother liquor to prepare pure Lithium Carbonate, described technique
Method flow is as it is shown in figure 1, carry out in accordance with the following steps:
S101: acidifying: add sulphuric acid in sinker mother solution, regulation, to PH=3, is subsequently adding liquid caustic soda, regulates to PH=7；
S102: fluorination sinker: the sodium fluoride adding excess 8% in the solution in described step S101 carries out sinker reaction, then
Solid-liquor separation, obtains lithium fluoride slag；
S103: causticization of sizing mixing: adding pure water in described lithium fluoride slag and size mixing, the pure water of addition is liquid-solid with lithium fluoride slag
Ratio is 30:1, adds calcium hydroxide and carries out causticizing reaction, then filter, obtain lithium hydroxide solution after sizing mixing；
S104: hydrogenation: be passed through carbon dioxide in described lithium hydroxide solution and carry out hydrogenation, obtain lithium bicarbonate molten
Liquid；
S105: Thermal desorption lithium: described lithia water heating 90 DEG C is decomposed, separates out pure Lithium Carbonate.
As seen from the above table, the lithium carbonate that embodiment 1 to embodiment 3 prepares all reaches high-purity grade standard, therefore, uses this
The lithium carbonate that the process utilizing battery-level lithium carbonate sinker disposing mother liquor to prepare pure Lithium Carbonate of bright offer prepares can be straight
Access high-purity level, it is not necessary to sinker mother solution return original system is first prepared technical grade lithium carbonate, then by technical grade lithium carbonate through severe
Changing and prepare pure Lithium Carbonate after obtaining Lithium hydrate, technique is simple, low cost, has broken female only with LITHIUM BATTERY sinker at present
Liquid prepares the commercial routes of the other lithium carbonate of lower level, and prepares the pure Lithium Carbonate of wellr sold and in short supply higher value, economic benefit
Considerable, it is suitable for industrial applications.
The above is only the detailed description of the invention of the present invention, makes to skilled artisans appreciate that or realize this
Bright.Multiple amendment to these embodiments will be apparent to one skilled in the art, as defined herein
General Principle can realize without departing from the spirit or scope of the present invention in other embodiments.Therefore, the present invention
It is not intended to be limited to the embodiments shown herein, and is to fit to and principles disclosed herein and features of novelty phase one
The widest scope caused.
Claims (4)
1. one kind utilizes the technique that battery-level lithium carbonate sinker disposing mother liquor prepares pure Lithium Carbonate, it is characterised in that described work
Process is carried out as follows:
S101: acidifying: add sulphuric acid in sinker mother solution, regulate PH=2-5, be subsequently adding liquid caustic soda or solid caustic soda, regulate PH=
7-8；
S102: fluorination sinker: add sodium fluoride in the solution in described step S101 and carry out sinker reaction, the most liquid-solid point
From, obtain lithium fluoride slag；
S103: causticization of sizing mixing: add pure water in described lithium fluoride slag and size mixing, add calcium hydroxide after sizing mixing and carry out causticization
Reaction, then filters, and obtains lithium hydroxide solution；
S104: hydrogenation: be passed through carbon dioxide in described lithium hydroxide solution and carry out hydrogenation, obtain lithium bicarbonate molten
Liquid；
S105: Thermal desorption lithium: by described lithia water heat resolve, separates out pure Lithium Carbonate.
The technique utilizing battery-level lithium carbonate sinker disposing mother liquor to prepare pure Lithium Carbonate the most according to claim 1, its
It is characterised by, described step S102 adds the amount of sodium fluoride than Li in the solution of described step S101+Required theoretical amount excess
5%-8%。
The technique utilizing battery-level lithium carbonate sinker disposing mother liquor to prepare pure Lithium Carbonate the most according to claim 1, its
Being characterised by, the pure water added in described step S103 is 20-30:1 with the liquid-solid ratio of lithium fluoride slag.
The technique utilizing battery-level lithium carbonate sinker disposing mother liquor to prepare pure Lithium Carbonate the most according to claim 1, its
Being characterised by, in described step S105, heating-up temperature is more than 90 DEG C.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107128954A (en) * | 2017-03-01 | 2017-09-05 | 衢州永东化工有限公司 | A kind of method for producing LITHIUM BATTERY lithium hydroxide |
| CN107720789A (en) * | 2017-11-22 | 2018-02-23 | 大余县旭日矿业科技有限公司 | A kind of technique for preparing pure Lithium Carbonate using battery-level lithium carbonate sinker disposing mother liquor |
| CN109264747A (en) * | 2018-09-29 | 2019-01-25 | 广东邦普循环科技有限公司 | A method of lithium hydroxide is prepared with the fluorination slag containing lithium |
| CN109399673A (en) * | 2018-12-25 | 2019-03-01 | 江西东鹏新材料有限责任公司 | Lithia water decomposition method |
| CN110104665A (en) * | 2019-03-13 | 2019-08-09 | 江西赣锋锂业股份有限公司 | A method of lithium carbonate is prepared using lithium fluoride waste liquid |
| CN110668473A (en) * | 2019-08-13 | 2020-01-10 | 中国科学院过程工程研究所 | Method for recovering lithium from waste lithium ion battery negative electrode material |
| CN111533144A (en) * | 2020-03-27 | 2020-08-14 | 白银中天化工有限责任公司 | Method for purifying low-grade lithium fluoride |
| CN111589278A (en) * | 2020-04-27 | 2020-08-28 | 湖南凯地众能科技有限公司 | System and method for recycling water of recovered waste lithium ion battery |
| CN111994924A (en) * | 2020-09-09 | 2020-11-27 | 江西云锂材料股份有限公司 | Novel method for producing high-purity lithium fluoride by taking industrial-grade lithium carbonate as raw material |
| CN112573545A (en) * | 2020-12-25 | 2021-03-30 | 江苏容汇通用锂业股份有限公司 | Method for preparing microporous lithium fluoride |
| CN114105172A (en) * | 2021-12-20 | 2022-03-01 | 福州大学 | Method for producing high-purity lithium carbonate by causticizing and carbonizing rough lithium carbonate lime |
| WO2023246156A1 (en) * | 2022-06-20 | 2023-12-28 | 广东邦普循环科技有限公司 | Process for preparing lithium hydroxide by causticization and use thereof |
| WO2024040907A1 (en) * | 2022-08-25 | 2024-02-29 | 广东邦普循环科技有限公司 | Preparation method for battery-grade lithium carbonate |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107128954A (en) * | 2017-03-01 | 2017-09-05 | 衢州永东化工有限公司 | A kind of method for producing LITHIUM BATTERY lithium hydroxide |
| CN107720789A (en) * | 2017-11-22 | 2018-02-23 | 大余县旭日矿业科技有限公司 | A kind of technique for preparing pure Lithium Carbonate using battery-level lithium carbonate sinker disposing mother liquor |
| CN109264747B (en) * | 2018-09-29 | 2021-08-03 | 广东邦普循环科技有限公司 | Method for preparing lithium hydroxide from lithium-containing fluorinated slag |
| CN109264747A (en) * | 2018-09-29 | 2019-01-25 | 广东邦普循环科技有限公司 | A method of lithium hydroxide is prepared with the fluorination slag containing lithium |
| CN109399673A (en) * | 2018-12-25 | 2019-03-01 | 江西东鹏新材料有限责任公司 | Lithia water decomposition method |
| CN110104665A (en) * | 2019-03-13 | 2019-08-09 | 江西赣锋锂业股份有限公司 | A method of lithium carbonate is prepared using lithium fluoride waste liquid |
| CN110104665B (en) * | 2019-03-13 | 2021-10-01 | 新余赣锋锂业有限公司 | Method for preparing lithium carbonate by using lithium fluoride waste liquid |
| CN110668473A (en) * | 2019-08-13 | 2020-01-10 | 中国科学院过程工程研究所 | Method for recovering lithium from waste lithium ion battery negative electrode material |
| CN111533144A (en) * | 2020-03-27 | 2020-08-14 | 白银中天化工有限责任公司 | Method for purifying low-grade lithium fluoride |
| CN111589278A (en) * | 2020-04-27 | 2020-08-28 | 湖南凯地众能科技有限公司 | System and method for recycling water of recovered waste lithium ion battery |
| CN111994924A (en) * | 2020-09-09 | 2020-11-27 | 江西云锂材料股份有限公司 | Novel method for producing high-purity lithium fluoride by taking industrial-grade lithium carbonate as raw material |
| CN112573545A (en) * | 2020-12-25 | 2021-03-30 | 江苏容汇通用锂业股份有限公司 | Method for preparing microporous lithium fluoride |
| CN114105172A (en) * | 2021-12-20 | 2022-03-01 | 福州大学 | Method for producing high-purity lithium carbonate by causticizing and carbonizing rough lithium carbonate lime |
| CN114105172B (en) * | 2021-12-20 | 2023-11-14 | 福州大学 | Method for producing high-purity lithium carbonate by causticizing and carbonizing crude lithium carbonate lime |
| WO2023246156A1 (en) * | 2022-06-20 | 2023-12-28 | 广东邦普循环科技有限公司 | Process for preparing lithium hydroxide by causticization and use thereof |
| WO2024040907A1 (en) * | 2022-08-25 | 2024-02-29 | 广东邦普循环科技有限公司 | Preparation method for battery-grade lithium carbonate |
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Denomination of invention: A process for preparation of high purity lithium carbonate by recovering the mother liquor of battery grade lithium carbonate precipitation Effective date of registration: 20200928 Granted publication date: 20180130 Pledgee: Feicheng City Assets Management Co.,Ltd. Pledgor: SHANDONG RUIFU LITHIUM INDUSTRY Co.,Ltd. Registration number: Y2020980006546 |
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